反应 #164522

ord-054d4a7a395e4bf7aa1e7ee4c889894b

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction was refluxed for 13 hrs
  2. 2
    温度at reflux temperature
  3. 3
    workup.DISTILLATIONThe solvent was distilled off
  4. 4
    其他to get the light brown solid product with a melting point of 58° C

实验过程

2-hydroxymethyl-8-phenethyl-1,4-dioxa-8-azaspiro[4,5]decane (Compound 1, 50 gm, 0.18 mole) and Para Toluenesulfonic Acid (PTSA, 2 gm) were dissolved in toluene (350 ml) at room temperature. 20 gm of thiophenol was added drop wise to the above solution. The reaction was refluxed for 13 hrs at reflux temperature. The solvent was distilled off to get the light brown solid product with a melting point of 58° C. The yield of the product was 95%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08841296B2uspto-grants-2014_09